2-Nitroanisole → Methyl alpha-chloro-3-methoxy-4-nitrophenylacetate

HRID 1018011

반응식

HRID 1018011 반응식
CC(C)([O-])C.[K+].[N+:7]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[O:16][CH3:17])([O-:9])=[O:8].[Cl:18][CH:19](Cl)[C:20]([O:22][CH3:23])=[O:21]>C(O)(=O)C>[Cl:18][CH:19]([C:13]1[CH:14]=[CH:15][C:10]([N+:7]([O-:9])=[O:8])=[C:11]([O:16][CH3:17])[CH:12]=1)[C:20]([O:22][CH3:23])=[O:21]

참가 물질

5

반응물 3

HCID 70482-NitroanisoleHCID 8315Methyl dichloroacetateHCID 23665647Potassium tert-butoxide

생성물 1

HCID 10061131Methyl alpha-chloro-3-methoxy-4-nitrophenylacetate

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A suspension of potassium t-butoxide (1.44 kg) in dimethylformamide(6.61) cooled to −5° C. to −10° C., was treated with a mixture of 2-nitroanisole (690 g) and methyl dichloroacetate (915 g) over 4 hours, whilst maintaining the temperature below −5° C. The reaction mixture was then treated with acetic acid (770 ml) and then with water (6.61) and then e extracted three times with tert-butyl methyl ether (5.51). The combined extracts were washed with water (5.51), then with saturated sodium bicarbonate solution (5.51), then with saturated brine (5.51) and then dried over magnesium sulphate to give a solution of methyl α-chloro-3-methoxy-4-nitrophenylacetate.

후처리

  1. temperaturecooled to −5° C. to −10° C.
  2. temperaturewhilst maintaining the temperature below −5° C
  3. extractionwith water (6.61) and then e extracted three times with tert-butyl methyl ether (5.51)
  4. washThe combined extracts were washed with water (5.51)
  5. dry with materialwith saturated sodium bicarbonate solution (5.51), then with saturated brine (5.51) and then dried over magnesium sulphate

출처 및 근거

ORD 기록
ord-4c4a2c05aa8c49e4a858341b89cd98bd
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06479519B1

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